Introduction to VDA-19.

1 and ISO-16232

Cleanliness control
Particular contamination

Dr. Markus J. Heneka, Dr. Sebastian Wex

Contaminants on Surface
Particulate and Filmic Contamination Go Together

Particulate contamination Filmic contamination

Filmic contamination provides

adhesion for particles

[VDA-19.1]

Particulate contamination : Solid granular particles und fibers

Filmic contamination : Thin layer of oily, waxy or greasy compounds

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 2

Contamination Categories
Typical Contaminants Found on Component Surface

Particulate Contamination Filmic

Minerals Metals Salts Organic Oil/ Grease

hard soft

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 3

Standardized Cleanliness Testing
ISO-16232 and VDA-19.1 are the Most Common Directives World-Wide

What is regulated in the norms?

• Selection of methods approved for testing

• How to apply and validate the test methods

What is not regulated?

• Which test method is suitable for a specific part

• Which cleanliness level to apply for a specific part

→ See customer requirement

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 4

Cleanliness Testing Overview
Three-Step Approach Standardized in VDA-19.1 and ISO-16232

1 Extraction of particles from component surface

Filtration of contaminant particles on a membrane

2

3 Analysis of contaminant particles (mass, size, numbers and type)

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 5

Cleanliness Testing Overview
Three-Step Approach Standardized in VDA-19.1 and ISO-16232

Liquid extraction Air extraction

1 Pressure-rinsing Internal rinsing Air jet extraction

Ultrasound Agitation Air throughflow extraction

2 Analysis filtration

Light optical from 50 µm Light optical from 5 µm SEM-EDX

Gravimetric Raman spectroscopy IR spectroscopy

3 Micro-CT LIBS
Standard analysis

Extended analysis

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 6

Particle Extraction
Rinsing with Pressurised Liquid Jet

Starting Parameters (ISO-16232)

Application
• Volume flow: 1.5 l/min
• Fluid volume: 5 ml/cm2
• Distance: max. 15 cm
Single components
Large surfaces
• Nozzle shape, diameter: round, 2.5 mm

Use cabinet or laboratory equipment

Small parts

Interior surfaces

[VDA-19.1] [C.Roth]
[Hydac]

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 7

Particle Extraction
Rinsing with Pressurised Liquid Jet

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 8

Particle Extraction
Ultrasonic Vibration

Application Starting Parameters (ISO-16232)

• Frequency 35-40 kHz
• Power density 10 Watts/liter
• Duration 30-60 sec

Small parts in beaker Use cabinet or laboratory equipment

Small parts in basket

Single components

[VDA-19.1] [Sonorex]
[Hydac]

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 9

Particle Extraction
Ultrasonic Vibration

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 10

Particle Extraction
Internal Rinsing by Liquid Flow

Application Starting Parameters (ISO-16232)

• Volume flow 1-20 l/min (turbulent)
• Duration 15-60 sec
• Pulsation, reversal of direction

Bores, feedthroughs Pipes, tubes Use cabinet or laboratory equipment

Coolers, housings

[VDA-19.1] [Sartorius]
[Hydac]

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 11

Particle Extraction
Agitation by Shaking

Application Starting Parameters (ISO-16232)

• Volume filling 40-50%
• Amplitude 30 cm, Frequency 1 Hz
• Time 15-60 sec

Containers Pressure tanks Use cabinet or laboratory equipment

Do not!

Large tubes Small components

[VDA-19.1]

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 12

Cleanliness Testing Overview
Three-Step Approach Standardized in VDA-19.1 and ISO-16232

Liquid extraction Air extraction

1 Pressure-rinsing Internal rinsing Air jet extraction

Ultrasound Agitation Air throughflow extraction

2 Analysis filtration

Light optical from 50 µm Light optical from 5 µm SEM-EDX

Gravimetric Raman spectroscopy IR spectroscopy

3 Micro-CT LIBS
Standard analysis

Extended analysis

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 13

Analysis filtration
Direct-Filtration

filtration funnel

analysis filter

Filter holder

[Hydac]

Vacuum source [VDA-19]

Cleaning cabinet

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 14

Analysis Filtration
Deposition of Contaminants on a Membrane by Vacuum Filtration

Filtration funnel
Analysis filter

Filter holder

Vacuum source

Vacuum flask

Laboratory equipment for vacuum filtration

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 15

Analysis Filtration
Vacuum Filtration Unit

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 16

Drying of Membrane
Preparation for filter analysis

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 17

Analysis filtration
Well-prepared membrane

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 18

Cleanliness Testing Overview
Three-Step Approach Standardized in VDA-19.1 and ISO-16232

Liquid extraction Air extraction

1 Pressure-rinsing Internal rinsing Air jet extraction

Ultrasound Agitation Air throughflow extraction

2 Analysis filtration

Light optical from 50 µm Light optical from 5 µm SEM-EDX

Gravimetric Raman spectroscopy IR spectroscopy

3 Micro-CT LIBS
Standard analysis

Extended analysis

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 19

Cleanliness Specifications
Typical Requirements from the Customer

Particle mass Particle size Particle material

Example: Example: Example:

Total particle mass less No particles larger than No abrasive particles of
than 5 mg per 1000 cm². 400 microns allowed, soft quartz, corundum, silicon
fibers are tolerated. carbide allowed larger
than 100 µm.

test complexity – equipment cost

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 20

Gravimetry
Determination of Particle weight

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 21

Standard Analysis
Determination of Particle Size and Number By Microscope or Scanner

Standard Analysis
> 50 µm

[Leica]

[Zeiss]

[RJL]

Particle size

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 22

Standard Analysis
Typical Cleanliness Report on Three Pages

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 23

Comparison to Light Microscopy
Light-optical analysis using a light microscope or scanner

particle scanner light microscope

• Particles > 25 µm • Particles > 5 µm (model dependant)
• fast (2 minutes + reporting) • widely used standard
• low investment, maintenance free • high image quality, variable magnification
• Imaging of entire membrane • sequential analysis of fields, stitching

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 24

Comparison to Light Microscopy
Excellent Correlation of MicroQuick and Five Light Microscopes (6/2014)

MicroQuick (green bar)

others: Leica, Zeiss, Jomesa

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 25

Identification of Metallic Particles
Determination of Particle Material by SEM-EDX

Electron Microscopy (SEM) with X-Ray Spectroscopy (EDX)

• automated measuring of particle size,

number and material
• smallest particles from 0.5 µm
• Determination of origin of particles
gezählte Röntgenquanten

Peak-Height =
Weight proportion

[FEI]

X-ray energy (keV)

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 26

Automatische Partikelanalyse
Aspex Automated Feature Analysis (AFA) im Video
Steels

Coatings

Non-ferrous metals

Abrasive Minerals

Cleaner

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 27

RJL Micro & Analytic GmbH
Analysis Services & Instruments | From One Source

Product Lines
Particle Scanner (MicroQuick)
Compact SEM-EDX (Coxem)
X-Ray Micro & Nano-CT (Bruker)
Digital 2D X-Ray Imaging (Kubtec)

Contract Analyses
Cleanliness Testing
Determination of Foreign Particles
With Accreditation DIN EN ISO/IEC 17025
Karlsruhe

© ∙ 76689 Karlsdorf-Neuthard ∙ Germany 28